CN114875247B - Method for treating three-phase substances in copper extraction process - Google Patents

Method for treating three-phase substances in copper extraction process Download PDF

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CN114875247B
CN114875247B CN202210458884.XA CN202210458884A CN114875247B CN 114875247 B CN114875247 B CN 114875247B CN 202210458884 A CN202210458884 A CN 202210458884A CN 114875247 B CN114875247 B CN 114875247B
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phase
slag
content
oil
water
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CN114875247A (en
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倪潇
邹潜
周艳红
王永茜
汤启明
徐志刚
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Chongqing Kopper Chemical Industry Co ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00Obtaining copper
    • C22B15/0063Hydrometallurgy
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The application relates to the technical field of hydrometallurgy, and discloses a method for treating three-phase substances in a copper extraction process, which comprises the following steps: step one: detecting the concentration of a three-phase substance stock solution; step two: and (3) separating, namely determining separating conditions according to the detection result, and feeding the three-phase substance stock solution into a three-phase horizontal spiral centrifuge to separate the water phase, the oil phase and the slag. The application adopts a three-phase horizontal spiral centrifuge to replace a plate-and-frame filter press of the current treatment process, and can separate collected three-phase substances to obtain a water phase, an organic phase and solid slag by only adopting a single horizontal spiral centrifuge. The whole production is continuous, airtight and automatic, activated clay, diatomite and the like are not needed, the amount of generated waste slag is small, the organic content is very low, the operation intensity of workers is reduced, and the environmental sanitation of workshops is improved.

Description

Method for treating three-phase substances in copper extraction process
Technical Field
The application relates to the technical field of hydrometallurgy, in particular to a method for treating three-phase substances in a copper extraction process.
Background
In copper extraction processes, three phases of material are inevitably present. The three-phase material is heavier than the organic phase and lighter than the water phase, and mainly comprises the organic phase, water, solid particles and entrained air. Its occurrence has a negative impact on the overall copper extraction process, so that the copper wet plant has to handle the three-phase material. The existing treatment method is to adopt a plate-and-frame filter press for filter pressing, wherein after three phases of activated clay are subjected to filter pressing, liquid phase enters a clarification tank to separate water and oil phases. The traditional treatment method has small treatment capacity, the plate-and-frame filter press is operated intermittently, and the operation time is long. The filtrate is difficult to avoid dripping and splashing in the filtration, the environment of a filtrate workshop is difficult to ensure, and the discharge of filter cakes requires manual operation by workers, so that the labor intensity is high. The three-phase separation in the filter pressing operation is not thorough, and the generated slag phase has high water content and oil content and takes away the organic phase. The filter cloth is often blocked in the filter pressing of activated clay in the prior art, manual cleaning is needed, the solid slag yield is high, and the cost for treating hazardous waste is high.
Disclosure of Invention
The application aims to provide a treatment method of three-phase substances in a copper extraction process, which aims to solve the problem that the separation of the three-phase substances is not thorough in the prior art.
In order to achieve the above purpose, the application adopts the following technical scheme: a method for treating three-phase substances in a copper extraction process comprises the following steps:
step one: detecting the concentration of a three-phase substance stock solution;
step two: and (3) separating, namely determining separating conditions according to the detection result, and feeding the three-phase substance stock solution into a three-phase horizontal spiral centrifuge to separate the water phase, the oil phase and the slag.
The principle and the advantages of the scheme are as follows: because the oil content in the oil, water and slag three-phase substances is higher, the three-phase substances are greatly different from the common municipal sludge, food residues and kitchen sewage. In the prior art, two centrifuges are usually required for separating oil, water and slag three-phase substances, the first centrifuges separate a solid phase and two liquid phases (aqueous phase and oil phase) firstly, then the second centrifuges separate the two liquid phases, and activated clay is additionally added before separation, so that the amount of the treated waste slag not only contains solid slag in the three-phase substances, but also contains the added activated clay, and the amount of the solid slag and the subsequent treatment difficulty are increased. The technical scheme adopts a three-phase horizontal spiral centrifuge to replace a plate-and-frame filter press of the current treatment process, and can separate collected three-phase substances into a water phase, an organic phase and solid slag by only adopting a single horizontal spiral centrifuge, so that conditions are optimized without additionally adding activated clay, and in addition, through practical verification, the scheme can also shorten the separation time of the three-phase substances, and has remarkable effect. When the three-phase horizontal spiral centrifugal machine is used for separating three-phase substances, the stock solution of the three-phase substances to be separated is sent into the rotary drum through the hollow rotating shaft and is immediately thrown into the cavity of the rotary drum under the centrifugal force generated by high-speed rotation. The high-speed rotating drum generates strong centrifugal force to throw solid-phase particles with higher density than liquid phase onto the inner wall of the drum to form a solid layer (called a solid ring layer because of ring shape). There is relative movement (i.e., a difference in rotational speed) between the screw conveyor and the rotating drum due to the difference in rotational speed. The sludge in the solid ring layer can be slowly pushed to the cone end of the rotary drum by utilizing the relative motion of the spiral conveyor and the rotary drum, and is continuously discharged from outlets distributed on the circumference of the rotary drum after passing through the drying area, so that slag discharge treatment is realized, and the part is used as dangerous waste to enter the subsequent treatment step. And two liquid phases (water phase and oil phase) with different densities form a concentric cylinder, wherein a lighter liquid phase is positioned in an inner layer, and a heavier liquid phase is positioned in an outer layer. The liquid in the liquid ring layer is discharged to the outside of the rotary drum by gravity through the weir to form separating liquid, the water phase returns to the extraction system, and the oil phase is recycled. The whole production is continuous, airtight and automatic, activated clay, diatomite and the like are not needed, the amount of generated waste slag is small, the organic content is very low, the operation intensity of workers is reduced, and the environmental sanitation of workshops is improved.
Preferably, in the second step, the three-phase horizontal spiral centrifuge comprises a rotary drum, a spiral conveyor and a differential mechanism, wherein the spiral conveyor is coaxially arranged with the rotary drum, a main shaft of the spiral conveyor is arranged as a hollow shaft, and the rotating speed of the spiral conveyor is smaller than that of the rotary drum.
In the technical scheme, the structure of the three-phase horizontal spiral centrifugal machine is basically the same as that of the prior art, equipment does not need to be structurally adjusted, and when the three-phase horizontal spiral centrifugal machine is used, effective separation of three-phase substances is realized, and the key points and the difficulty lie in frequency optimization, namely rotation speed optimization.
Preferably, as an improvement, in the second step, when the moisture content of the three-phase substances to be detected is less than 10.25%, the main machine frequency and the auxiliary machine frequency of the three-phase horizontal spiral centrifugal machine are respectively 24-30HZ and 18-25HZ.
According to the technical scheme, after the concentration of the stock solution of the three-phase substances to be separated is analyzed, when the concentration of the stock solution of the three-phase substances to be separated is low, the frequency of a main machine is controlled to be 24-30HZ, the frequency of an auxiliary machine is controlled to be 18-25HZ, the water content in oil discharged by the separation method of the scheme can be ensured to be less than 0.04%, the wet slag content is 0.006%, water and slag are hardly contained in an organic phase after treatment, slag discharge is relatively dry, and the transfer is convenient for waste treatment.
Preferably, as an improvement, in the second step, when the moisture content of the three-phase substances to be detected is 10.25-38.43%, the main machine frequency and the auxiliary machine frequency of the three-phase horizontal spiral centrifuge are respectively 30-33HZ and 25-28HZ.
According to the technical scheme, after the concentration of the stock solution of the three-phase substances to be separated is analyzed, when the three-phase substances to be separated are of medium concentration, the frequency of a main machine and a secondary machine is optimized, centrifugal separation is respectively carried out under the conditions of the frequency of the main machine and the secondary machine of 30HZ-25HZ and 33HZ-28HZ, the results show that the water content in oil is less than 0.04%, the slag content of 33HZ-28HZ is 0.090%, the 30HZ-25HZ is 0.028%, the slag content of the oil is very small, and the treated oil is almost free of water and slag, and the oil is sufficiently separated from water and three phases.
Preferably, as an improvement, in the second step, when the moisture content of the three-phase substance to be detected is 38.43-42.66%, the main machine frequency and the auxiliary machine frequency of the three-phase horizontal spiral centrifuge are 33-36HZ and 28-31HZ respectively.
In the technical scheme, after the concentration of the stock solution of the three-phase substances to be separated is analyzed, when the concentration of the three-phase substances to be separated is high, the frequency of the main machine and the auxiliary machine is optimized, and centrifugal separation is carried out under the conditions of the frequency of the main machine and the auxiliary machine of 30HZ-25HZ, 33HZ-28HZ and 36HZ-31HZ, and the result shows that: the oil content of the effluent is less than 0.04% at three frequencies, so that the oil-water separation is more complete; the slag content of the water discharged at the three frequencies is 8.17%, 18.55% and 26.58% in sequence, and the higher the centrifugal frequency is, the more favorable the separation of water and three phases is.
Preferably, as an improvement, in the second step, when the moisture content of the three-phase substance to be detected is less than 10.25%, the main machine frequency and the auxiliary machine frequency of the three-phase horizontal spiral centrifuge are respectively 28HZ and 23HZ.
In the technical scheme, when the low-concentration three-phase substances are separated, experiments prove that the optimal main machine frequency and auxiliary machine frequency are respectively 28HZ and 23HZ, so that the separation effect can be ensured, and unnecessary energy consumption can be avoided.
Preferably, as an improvement, in the second step, when the moisture content of the three-phase substance to be detected is 10.25-38.43%, the main machine frequency and the auxiliary machine frequency of the three-phase horizontal spiral centrifuge are respectively 33HZ and 28HZ.
In the technical scheme, when separating the medium-concentration three-phase material stock solution, the frequency is increased from the main machine 30HZ and the auxiliary machine 25HZ to the main machine 33HZ and the auxiliary machine 28HZ, the slag content in the discharged water can be obviously reduced, the water content in the slag is reduced in a proper amount, and the main machine 33HZ and the auxiliary machine 28HZ are selected to treat the medium-concentration three-phase solution, so that the medium-concentration three-phase solution has a good separation effect.
Preferably, as an improvement, in the second step, when the moisture content of the three-phase substance to be detected is 38.43-42.66%, the main machine frequency and the auxiliary machine frequency of the three-phase horizontal spiral centrifuge are 33HZ and 28HZ respectively.
In the technical scheme, the separation conditions of the high-concentration three-phase material stock solution are optimized, the water content of the slag is 42.60%, 42.11% and 44.82% in sequence under three frequencies, the slag is drier, and the increase of the frequency of the centrifugal machine has no obvious effect on improving and reducing the water content of the slag. The frequency is increased from the main machine 30HZ and the auxiliary machine 25HZ to the main machine 36HZ and the auxiliary machine 31HZ, which has no great effect on reducing the water content in slag, but can obviously reduce the slag content in the effluent, and the frequency separation effect of the main machine 33HZ and the auxiliary machine 28HZ for treating high-concentration three-phase liquid is better.
Drawings
FIG. 1 is a flow chart showing the process of the three-phase material according to example 1 of the present application.
Detailed Description
The following is a further detailed description of the embodiments:
the scheme is as follows:
the three-phase horizontal spiral centrifugal machine is basically as the structure of the prior art, and mainly comprises a rotary drum, a rotary drum with high rotating speed, a spiral conveyor with a hollow rotating shaft, a differential mechanism and the like, wherein the rotary drum is identical in rotation direction with the rotary drum, and the rotary speed of the spiral conveyor is slightly lower than that of the rotary drum.
As shown in figure 1, when the three-phase horizontal spiral centrifugal machine is used for separating three-phase substances, the stock solution of the three-phase substances to be separated is sent into the rotary drum through the hollow rotating shaft and is immediately thrown into the cavity of the rotary drum under the centrifugal force generated by high-speed rotation. The high-speed rotating drum generates strong centrifugal force to throw solid-phase particles with higher density than liquid phase onto the inner wall of the drum to form a solid layer (called a solid ring layer because of ring shape). There is relative movement (i.e., a difference in rotational speed) between the screw conveyor and the rotating drum due to the difference in rotational speed. The sludge in the solid ring layer can be slowly pushed to the cone end of the rotary drum by utilizing the relative motion of the spiral conveyor and the rotary drum, and is continuously discharged from outlets distributed on the circumference of the rotary drum after passing through the drying area, so that slag discharge treatment is realized, and the part is used as dangerous waste to enter the subsequent treatment step. And two liquid phases (water phase and oil phase) with different densities form a concentric cylinder, wherein a lighter liquid phase is positioned in an inner layer, and a heavier liquid phase is positioned in an outer layer. The liquid in the liquid ring layer is discharged to the outside of the rotary drum by gravity through the weir to form separating liquid, the water phase returns to the extraction system, and the oil phase is recycled.
EXAMPLE 1 Low concentration three-phase stock solution treatment
The wet slag content of the low-concentration three-phase liquid is 10.25%, the main machine frequency and the auxiliary machine frequency are respectively 24-30HZ and 18-25HZ, and the water content, the oil content and the slag content of the oil outlet, the water outlet and the slag outlet are shown in the following table 1. The oil content in the water phase is centrifugated for 20min at a rotating speed of 2000rpm by high-speed centrifugation, oil drops in the water are separated by supergravity, then the water phase is kept stand for 2min, and the weight of the oil phase is calculated by liquid separation. The solids content in the aqueous phase was obtained by filtration (using 2.5 μm aqueous filter paper for filtration) and then weighed. The oil content in the oil phase was determined by the Tokarl-Fischer method. The solids content in the oil phase was obtained by filtration (using 2.5 μm oily filter paper for filtration) and then weighed. The water content in the slag is measured by a low-temperature weightlessness method, dried for more than 8 hours at 95 ℃, and then weighed.
TABLE 1
Detection item Moisture content (%) Oil content (%) Wet residue (%) Dry slag (%)
Low concentration stock solution 16.15 72.80 10.25 1.51
Low concentration oil outlet <0.04 / 0.006 <0.04
Low concentration effluent / <0.04 15.27 1.57
Low concentration slag tap 46.52 / / /
The oil output data shows that the water content in the oil output (oil phase after separation) is less than 0.04%, the wet slag content is 0.006%, and the organic phase after treatment contains almost no water and slag, so that the oil is fully separated from water and three phases. The effluent data show that the oil content in the effluent (separated water phase) is less than 0.04%, the wet slag content is 15.27%, and the effluent after treatment contains almost no oil, but contains a certain amount of three phases, so that the water and the oil are more sufficient, and part of the three phases are difficult to separate from the water after centrifugal scattering. The data of the slag (solid slag after separation) can show that the slag contains 46.52% of water, and the slag is dry and convenient to transfer for waste treatment. In conclusion, the low-concentration three-phase liquid has the advantages that oil separation is more complete, a small amount of three phases are carried in the effluent, slag is discharged more dry, the transfer is convenient for waste treatment, and the low-concentration three-phase liquid has a better separation effect.
Example 2 treatment of concentrated three-phase stock solution
The medium-concentration three-phase liquid wet slag content is 38.43%, and the data of water content, oil content and slag content of the oil, water and slag are shown in the following table 2 under the conditions of main and auxiliary machine frequencies of 30HZ (main) and 25HZ (auxiliary), 33HZ (main) and 28HZ (auxiliary). Wherein, the medium concentration oil outlet 33HZ-28HZ represents the oil phase of the medium concentration stock solution under the conditions of the main machine frequency 33HZ and the auxiliary machine frequency 28HZ.
TABLE 2
Detection item Moisture content (%) Oil content (%) Wet residue (%) Dry slag (%)
Medium concentration stock solution 56.22 4.58 38.43 28.27
Medium concentration oil 33HZ-28HZ <0.04 / 0.090 <0.04
Medium concentration oil outlet 30HZ-25HZ <0.04 / 0.028 <0.04
Medium concentration effluent 33HZ-28HZ / <0.04 27.33 6.29
Medium concentration effluent 30HZ-25HZ / <0.04 57.55 5.58
Medium concentration slag 33HZ-28HZ 41.44 / / /
Middle concentration slag tap 30HZ-25HZ 43.58 / / /
As shown in Table 2, the water content in the oil is less than 0.04%, the slag content is 33HZ-28HZ 0.090%, the slag content in the oil is 30HZ-25HZ 0.028%, and the oil slag content is small, which indicates that the oil contains almost no water and slag, and the oil is separated from water and three phases sufficiently. The oil content in the effluent is less than 0.04%, the slag content is 33HZ-28HZ (main machine-auxiliary machine) and is 27.33% which is half of 57.55% of 30HZ-25HZ, which shows that the effluent after treatment contains almost no oil, but contains a certain amount of three phases, and the slag content in the effluent can be effectively reduced by increasing the centrifugal frequency. The water content in the slag is 43.58% by weight, the water content in the slag is 41.44% by weight, and the slag is drier.
In summary, the centrifugal oil from the medium-concentration three-phase liquid still has a better separation effect, the frequency is increased from the main machine 30HZ and the auxiliary machine 25HZ to the main machine 33HZ and the auxiliary machine 28HZ, the slag content in the discharged water can be obviously reduced, the water content in the slag is reduced in a proper amount, and the medium-concentration three-phase liquid is treated by the main machine frequency 33HZ and the auxiliary machine frequency 28HZ, so that the separation effect is better.
EXAMPLE 3 high concentration three-phase stock solution treatment
The high-concentration three-phase liquid has a moisture content of 42.66%, and is subjected to centrifugal separation under the conditions of main-auxiliary machine frequencies of 30HZ-25HZ, 33HZ-28HZ and 36HZ-31HZ, and the data of water content, oil content and slag content of oil, water and slag are shown in the following table.
TABLE 3 Table 3
As shown in Table 3, the oil content of the effluent at three frequencies is less than 0.04%, and the oil-water separation is relatively sufficient; the slag content of the water discharged at the three frequencies is 8.17%, 18.55% and 26.58% in sequence, and the higher the centrifugal frequency is, the more favorable the separation of water and three phases is. The water content of the slag discharged under the three frequencies is 42.60%, 42.11% and 44.82% in sequence, the slag discharged is drier, and increasing the frequency of the centrifugal machine has no obvious effect on improving the reduction of the water content of the slag discharged.
In summary, the high-concentration three-phase liquid centrifugal oil outlet still has a better separation effect, the frequency is increased from the main machine 30HZ and the auxiliary machine 25HZ to the main machine 36HZ and the auxiliary machine 31HZ, the water content in the slag is reduced, but the slag content in the water outlet can be obviously reduced, and the frequency separation effect of the main machine 33HZ and the auxiliary machine 28HZ for treating the high-concentration three-phase liquid is better. In general, the horizontal decanter centrifuge is used for treating and extracting three phases, so that oil is relatively clean and can be directly returned to the system for use; the oil content in the effluent is lower than 0.04%, the slag content is increased under the influence of the frequency of a centrifugal machine, and the higher the centrifugal frequency is, the lower the slag content of the effluent is; the water content of the slag can reach below 50%, and the centrifugal frequency has no obvious influence on the water content of the slag.
Comparative example 1
In this comparative example, the three-phase stock solution to be separated had a water content of 25.18%, an oil content of 57.27%, and a wet slag content of 16.33% and a dry slag content of 3.09%, and the three-phase stock solution was treated by a conventional filter press, and the treatment results are shown in the following table. The three-phase liquid with low concentration (solid content) can be treated by adopting the filter press treatment, namely, the wet slag content is less than 20 percent.
TABLE 4 Table 4
Detection item Moisture content (%) Oil content (%) Wet residue (%) Dry slag (%)
Stock solution 25.18 57.27 16.33 3.09
Oil outlet 13.18 84.05 2.42 0.29
Filter residue pressing 41.22 / / /
Comparative example 2 Effect of frequency on separation effect and separation speed of three-phase substances
In the comparative experiment, high-concentration stock solution (the water content is 39.55%, the oil content is 15.20%, the wet slag is 42.66%, and the dry slag is 13.68%) is separated, separation effects and separation time under different main machine frequencies and auxiliary machine frequencies are explored, and specific experimental designs are shown in table 5.
TABLE 5
As can be seen from the data in table 5, in the present embodiment, when separating three-phase substances, not only the main machine frequency and the auxiliary machine frequency have a large influence on the separation effect, but also the proper main machine frequency and auxiliary machine frequency have a certain promotion effect on the separation time. When the frequency of the main machine and the frequency of the auxiliary machine are increased from 30HZ and 25HZ to 33HZ and 28HZ during separation, the separation time can be obviously shortened, and the frequency is continuously increased, so that the influence on the separation time is small.
The foregoing is merely exemplary of the present application, and specific technical solutions and/or features that are well known in the art have not been described in detail herein. It should be noted that, for those skilled in the art, several variations and modifications can be made without departing from the technical solution of the present application, and these should also be regarded as the protection scope of the present application, which does not affect the effect of the implementation of the present application and the practical applicability of the patent. The protection scope of the present application is subject to the content of the claims, and the description of the specific embodiments and the like in the specification can be used for explaining the content of the claims.

Claims (1)

1. The method for treating the three-phase substances in the copper extraction process is characterized by comprising the following steps of:
step one: detecting the concentration of a three-phase substance stock solution;
step two: separating, namely determining separating conditions according to a detection result, and feeding the three-phase substance stock solution into a three-phase horizontal spiral centrifuge to separate water phase, oil phase and slag charge during separating;
in the second step, the three-phase horizontal spiral centrifuge comprises a rotary drum, a spiral conveyer and a differential mechanism, wherein the spiral conveyer and the rotary drum are coaxially arranged, a main shaft of the spiral conveyer is arranged as a hollow shaft, and the rotating speed of the spiral conveyer is smaller than that of the rotary drum;
in the second step, when the moisture content of the three-phase substances to be detected is less than 10.25%, the main machine frequency and the auxiliary machine frequency of the three-phase horizontal spiral centrifuge are respectively 28Hz and 23Hz;
when the content of the wet slag of the three-phase substances to be detected is 10.25-38.43%, the main machine frequency and the auxiliary machine frequency of the three-phase horizontal spiral centrifuge are 33Hz and 28Hz respectively;
when the content of the wet slag of the three-phase substances to be detected is 38.43-42.66%, the main machine frequency and the auxiliary machine frequency of the three-phase horizontal spiral centrifugal machine are 33Hz and 28Hz respectively.
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